The goals of this project are focused on the evaluation of radiolabeled conjugates of the somatostatin analogue octreotide as therapeutic and diagnostic agents for cancers of the neuroendocrine system in both in vitro cell models and animal models. Conjugates of octreotide will be synthesized for the labeling of 64Cu and 68Ga to evaluate the potential for positron emission tomography (PET) imaging and radiotherapy. To radiolabel metal nuclides to octreotide, bifunctional chelates (BFC) must be designed and synthesized. Mass Spectrometry is needed to characterize the synthesized BFCs and their precursors. In the synthesis of these chelates, protection of thiols and amines is required. Mass spectrometry is a useful tool in determining the success of the protection and deprotection reactions.